A method for detecting total hydrocarbons

Abstract

The invention discloses a method for detecting total hydrocarbons. A method for detecting total hydrocarbons comprises the following steps: step 1, assembling a test pipeline; the test pipeline comprises a sample branch and a blank branch arranged in parallel, the sample branch and the blank branch are connected to a nitrogen supply pipeline through a three-way joint; the sample branch comprises a first gas pressure flow regulating component, a first butt-joint pipeline, a sample simulation component and a second butt-joint pipeline connected in sequence; the blank branch comprises a second gas pressure flow regulating component and a third butt-joint pipeline connected in sequence; step 2, heating and cleaning; placing the first butt-joint pipeline, the sample simulation component and the second butt-joint pipeline in an oven for heating; step 3, heating the sample branch and the blank branch; step 4, connecting the ends of the second butt-joint pipeline and the third butt-joint pipeline to an organic adsorption tube for sampling, and detecting the organic adsorption tube; step 5, installing the test sample for sampling; step 6, testing.

Description

Technical Field

[0001] The invention relates to the field of detection technology, in particular to a method for detecting hydrocarbons. Background Art

[0002] In semiconductor manufacturing, total organic carbon release is one of the key factors affecting the surface cleanliness of key components of semiconductor manufacturing equipment. There are limited methods to quickly, effectively and reasonably evaluate the hydrocarbons of metal parts.

[0003] There is an urgent need for a method that can take into account both the sampling equipment and the hydrocarbon content of the sampled gas to avoid bias in the hydrocarbon results of the tested parts. Summary of the invention

[0004] In view of the problems existing in the prior art, the present invention provides a method for detecting total hydrocarbons to solve at least one of the above technical problems.

[0005] In order to achieve the above object, the present invention provides a method for detecting total hydrocarbons, characterized in that it comprises the following steps:

[0006] Step 1: Assemble the test pipeline to ensure the air tightness of the pipeline;

[0007] The test pipeline comprises a sample branch and a blank branch arranged in parallel, and the sample branch and the blank branch are connected to a nitrogen supply pipeline through a three-way joint;

[0008] The sample branch includes a first air pressure flow regulating component, a first connecting pipe, a sample simulation component and a second connecting pipe connected in sequence;

[0009] The blank branch includes a second air pressure flow regulating component and a third connecting pipe connected in sequence;

[0010] Step 2: heating and cleaning;

[0011] Put the first pair of pipes, the sample dummy and the second pair of pipes into an oven for heating;

[0012] Step 3, heating the sample branch and the blank branch;

[0013] Step 4: Connect the ends of the second and third connecting pipes to the organic adsorption tubes for sampling, and test the organic adsorption tubes to ensure that the sample branch and the blank branch themselves are free of total hydrocarbons;

[0014] Step 5, remove the sample simulation part, install the test sample, and connect the two ends of the test sample to the first butt joint pipe and the second butt joint pipe respectively;

[0015] Connect the ends of the second and third pair of pipes to the organic matter adsorption tubes for sampling;

[0016] Step six, place the organic adsorption tube on the sample plate of TD-GCMS for testing.

[0017] Further preferably, in step 2, the temperature of the oven is 110° C., and the hot baking time of the oven is 60 min.

[0018] Further preferably, in step 3, the heating temperature is 70±2°C;

[0019] The first air pressure flow regulating component and the second air pressure flow regulating component control the flow rate at 0.9L / min-1.1L / min.

[0020] Further preferably, in step 5, the sample branch and the blank branch are heated, and the heating temperature is 70±2° C.;

[0021] The first air pressure flow regulating component and the second air pressure flow regulating component control the flow rate at 0.9L / min-1.1L / min.

[0022] Further preferably, in step three and step five, heating is performed by wrapping a heating tape around the outer sides of the sample branch and the blank branch.

[0023] Further preferably, in step three, a heating tape is wound around the pipeline area between the first air pressure flow regulating component and the sample;

[0024] Wrap a heating tape around the periphery of the third butting pipe.

[0025] Further preferably, the sample branch and the blank branch are wrapped around the same heating belt.

[0026] Further preferably, the first air pressure flow regulating component and the second air pressure flow component both include a first valve, a detection component and a second valve sequentially connected along the flow diversion direction, and the detection component includes a pressure gauge and a flow meter.

[0027] Further preferably, in step 5, the gas flow rate needs to be recorded before and after gas collection begins;

[0028] After step six, the sample data and blank data are calculated using the normalization method. The blank data is subtracted from the sample data and the data is quantified using the normalization method. The organic content is calculated with the volume of gas passing through to obtain the organic content in the component in ng / L.

[0029] A method for detecting total hydrocarbons, characterized in that it comprises the following steps:

[0030] Step 1: Assemble the test pipeline to ensure the air tightness of the pipeline;

[0031] The test pipeline comprises a sample branch and a blank branch arranged in parallel, and the sample branch and the blank branch are connected to a nitrogen supply pipeline through a three-way joint;

[0032] The sample branch includes a first air pressure flow regulating component, a first connecting pipe, a sample simulation component and a second connecting pipe connected in sequence;

[0033] The blank branch includes a second air pressure flow regulating component and a third connecting pipe connected in sequence;

[0034] The first air pressure flow regulating component and the second air pressure flow component each include a first valve, a detection component and a second valve sequentially connected along the flow diversion direction, and the detection component includes a pressure gauge and a flow meter;

[0035] Step 2: heating and cleaning;

[0036] Put the first pair of pipes, the sample dummy and the second pair of pipes into an oven for heating;

[0037] The temperature of the oven is 110°C, and the hot baking time of the oven is 60 minutes;

[0038] Step 3, heating the sample branch and the blank branch;

[0039] Wrap a heating tape around the outside of the sample branch and the blank branch for heating. The heating temperature of the heating tape is 70±2℃.

[0040] The first air pressure flow regulating component and the second air pressure flow regulating component control the flow rate to 0.9L / min-1.1L / min;

[0041] Step 4, connecting the ends of the second and third connecting pipes to the organic matter adsorption tube for sampling;

[0042] The nitrogen supply pipeline ventilates the sample branch and the blank branch for 1 hour, and the adsorption tubes connected to the second and third connecting pipelines collect gas for 1 hour;

[0043] Test the organic adsorption tube to ensure that there is no total hydrocarbon in the sample branch and the blank branch;

[0044] Step 5, remove the sample simulation part, install the test sample, and connect the two ends of the test sample to the first butt joint pipe and the second butt joint pipe respectively;

[0045] Keep the heating temperature of the heating belt at 70±2℃;

[0046] The first air pressure flow regulating component and the second air pressure flow regulating component control the flow rate to 0.9L / min-1.1L / min;

[0047] Connect the ends of the second and third pair of pipes to the organic matter adsorption tubes for sampling;

[0048] The nitrogen supply pipeline ventilates the sample branch and the blank branch for 1 hour, and the adsorption tubes connected to the second and third connecting pipelines collect gas for 1 hour;

[0049] Step six, place the organic adsorption tube on the sample plate of TD-GCMS for testing.

[0050] Beneficial effects: The present invention can effectively collect total hydrocarbons in parts and components, and can effectively analyze the types and contents in combination with TD-GCMS. BRIEF DESCRIPTION OF THE DRAWINGS

[0051] Figure 1 A structural schematic diagram of the present invention. DETAILED DESCRIPTION

[0052] The present invention will be further described below in conjunction with the accompanying drawings.

[0053] See also Figure 1 , Specific embodiment 1: A method for detecting total hydrocarbons, characterized in that it comprises the following steps:

[0054] Step 1: Assemble the test pipeline to ensure the air tightness of the pipeline;

[0055] The test pipeline comprises a sample branch and a blank branch arranged in parallel, and the sample branch and the blank branch are connected to a nitrogen supply pipeline 1 through a three-way joint;

[0056] The sample branch includes a first air pressure flow regulating component 2, a first connecting pipe 3, a sample simulation component 4 and a second connecting pipe 5 connected in sequence;

[0057] The blank branch includes a second air pressure flow regulating component 6 and a third connecting pipe 7 connected in sequence;

[0058] Step 2: heating and cleaning;

[0059] Put the first butt-jointed pipe 3, the sample dummy 4 and the second butt-jointed pipe 5 into an oven for heating;

[0060] Step 3, heating the sample branch and the blank branch;

[0061] Step 4: Connect the ends of the second connecting pipe 5 and the third connecting pipe 7 to the organic adsorption tube for sampling, and test the organic adsorption tube to ensure that there is no total hydrocarbon in the sample branch and the blank branch;

[0062] Step 5, remove the sample simulation part 4, install the test sample, and connect the two ends of the test sample to the first connecting pipe 3 and the second connecting pipe 5 respectively;

[0063] Connect the ends of the second connecting pipe 5 and the third connecting pipe 7 to the organic matter adsorption tube for sampling;

[0064] Step six, place the organic adsorption tube on the sample plate of TD-GCMS for testing.

[0065] In step 2, the temperature of the oven is 110° C., and the hot baking time of the oven is 60 min.

[0066] In step three, the heating temperature is 70±2° C.; the first air pressure flow regulating component 2 and the second air pressure flow regulating component 6 control the flow rate at 0.9 L / min-1.1 L / min.

[0067] In step five, the sample branch and the blank branch are heated to a temperature of 70±2° C.; the first air pressure flow regulating component 2 and the second air pressure flow regulating component 6 control the flow rate to 0.9 L / min-1.1 L / min.

[0068] In step 3 and step 5, heating is performed by wrapping a heating tape around the outside of the sample branch and the blank branch. In step 3, a heating tape is wrapped around the pipeline area between the first air pressure flow regulating component 2 and the sample; a heating tape is wrapped around the periphery of the third connecting pipeline 7. The sample branch and the blank branch are wrapped with the same heating tape.

[0069] The first air pressure flow regulating component 2 and the second air pressure flow component both include a first valve, a detection component and a second valve sequentially connected along the flow diversion direction, and the detection component includes a pressure gauge and a flow meter.

[0070] In step five, the gas flow rate needs to be recorded before and after the start of gas sampling; after step six, the normalization method is used to calculate the sample data and blank data, the blank data is deducted from the sample data, and the data is quantified by normalization method. The organic matter content is calculated with the volume of gas passing through, and the organic matter content in the component can be obtained in ng / L.

[0071] A method for detecting total hydrocarbons, characterized in that it comprises the following steps:

[0072] Step 1: Assemble the test pipeline to ensure the air tightness of the pipeline;

[0073] The test pipeline comprises a sample branch and a blank branch arranged in parallel, and the sample branch and the blank branch are connected to a nitrogen supply pipeline 1 through a three-way joint;

[0074] The sample branch includes a first air pressure flow regulating component 2, a first connecting pipe 3, a sample simulation component 4 and a second connecting pipe 5 connected in sequence;

[0075] The blank branch includes a second air pressure flow regulating component 6 and a third connecting pipe 7 connected in sequence;

[0076] The first air pressure flow regulating component 2 and the second air pressure flow component both include a first valve, a detection component and a second valve connected in sequence along the flow diversion direction, and the detection component includes a barometer and a flow meter;

[0077] Step 2: heating and cleaning;

[0078] Put the first butt-jointed pipe 3, the sample dummy 4 and the second butt-jointed pipe 5 into an oven for heating;

[0079] The temperature of the oven is 110°C, and the hot baking time of the oven is 60 minutes;

[0080] Step 3, heating the sample branch and the blank branch;

[0081] Wrap a heating tape around the outside of the sample branch and the blank branch for heating. The heating temperature of the heating tape is 70±2℃.

[0082] The first air pressure flow regulating component 2 and the second air pressure flow regulating component 6 control the flow rate at 0.9L / min-1.1L / min;

[0083] Step 4, connecting the ends of the second connecting pipe 5 and the third connecting pipe 7 to the organic adsorption tube for sampling;

[0084] The nitrogen supply pipeline 1 ventilates the sample branch and the blank branch for 1 hour, and the adsorption tubes connected to the second connecting pipeline 5 and the third connecting pipeline 7 collect gas for 1 hour;

[0085] Test the organic adsorption tube to ensure that there is no total hydrocarbon in the sample branch and the blank branch;

[0086] Step 5, remove the sample simulation part 4, install the test sample, and connect the two ends of the test sample to the first connecting pipe 3 and the second connecting pipe 5 respectively;

[0087] Keep the heating temperature of the heating belt at 70±2℃;

[0088] The first air pressure flow regulating component 2 and the second air pressure flow regulating component 6 control the flow rate at 0.9L / min-1.1L / min;

[0089] Connect the ends of the second connecting pipe 5 and the third connecting pipe 7 to the organic matter adsorption tube for sampling;

[0090] The nitrogen supply pipeline 1 ventilates the sample branch and the blank branch for 1 hour, and the adsorption tubes connected to the second connecting pipeline 5 and the third connecting pipeline 7 collect gas for 1 hour;

[0091] Step six, place the organic adsorption tube on the sample plate of TD-GCMS for testing.

[0092] The test results of a sample are as follows:

[0093] Total Concentration (ng / L) Hydrocarbons (>n-C6·to≤n-C9) ND Hydrocarbons (>n-C9·to≤n-C14) ND Hydrocarbons (>n-C14·to≤n-C20) 0.36 Hydrocarbons (>n-C20 to ≤n-C30) ND Total hydrocarbons (>n-C6·to≤n-C30) 0.36

[0094] The above are only preferred embodiments of the present invention. It should be pointed out that, for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for detecting total hydrocarbons, characterized in that: The steps include: Step 1: Assemble the test pipeline to ensure the air tightness of the pipeline; The test pipeline comprises a sample branch and a blank branch arranged in parallel, and the sample branch and the blank branch are connected to a nitrogen supply pipeline through a three-way joint; The sample branch includes a first air pressure flow regulating component, a first connecting pipe, a sample simulation component and a second connecting pipe connected in sequence; The blank branch includes a second air pressure flow regulating component and a third connecting pipe connected in sequence; Step 2: heating and cleaning; Put the first pair of pipes, the sample dummy and the second pair of pipes into an oven for heating; Step 3, heating the sample branch and the blank branch; Step 4: Connect the ends of the second and third connecting pipes to the organic adsorption tubes for sampling, and test the organic adsorption tubes to ensure that the sample branch and the blank branch themselves are free of total hydrocarbons; Step 5, remove the sample simulation part, install the test sample, and connect the two ends of the test sample to the first butt joint pipe and the second butt joint pipe respectively; Connect the ends of the second and third pair of pipes to the organic matter adsorption tubes for sampling; Step six, place the organic adsorption tube on the sample plate of TD-GCMS for testing.

2. The method for detecting total hydrocarbons according to claim 1, characterized in that: In step 2, the temperature of the oven is 110° C., and the hot baking time of the oven is 60 min.

3. The method for detecting total hydrocarbons according to claim 1, characterized in that: In step 3, the heating temperature is 70±2°C; The first air pressure flow regulating component and the second air pressure flow regulating component control the flow rate at 0.9L / min-1.1L / min.

4. The method for detecting total hydrocarbons according to claim 1, characterized in that: In step 5, the sample branch and the blank branch are heated at a temperature of 70±2°C; The first air pressure flow regulating component and the second air pressure flow regulating component control the flow rate at 0.9L / min-1.1L / min.

5. The method for detecting total hydrocarbons according to claim 1, characterized in that: In step 3 and step 5, heating is performed by wrapping a heating tape around the outside of the sample branch and the blank branch.

6. A method for detecting total hydrocarbons according to claim 5, characterized in that: In step three, a heating tape is wound around the pipeline area between the first air pressure flow regulating component and the sample; Wrap a heating tape around the periphery of the third butting pipe.

7. A method for detecting total hydrocarbons according to claim 6, characterized in that: The sample branch and the blank branch are wound around the same heating belt.

8. The method for detecting total hydrocarbons according to claim 1, characterized in that: The first air pressure flow regulating component and the second air pressure flow component both include a first valve, a detection component and a second valve sequentially connected along the flow diversion direction, and the detection component includes an air pressure meter and a flow meter.

9. The method for detecting total hydrocarbons according to claim 1, characterized in that: In step 5, the gas flow rate needs to be recorded before and after gas extraction begins; After step six, the sample data and blank data are calculated using the normalization method. The blank data is subtracted from the sample data and the data is quantified using the normalization method. The organic content is calculated with the volume of gas passing through to obtain the organic content in the component in ng / L.

10. A method for detecting total hydrocarbons, characterized in that: The steps include: Step 1: Assemble the test pipeline to ensure the air tightness of the pipeline; The test pipeline comprises a sample branch and a blank branch arranged in parallel, and the sample branch and the blank branch are connected to a nitrogen supply pipeline through a three-way joint; The sample branch includes a first air pressure flow regulating component, a first connecting pipe, a sample simulation component and a second connecting pipe connected in sequence; The blank branch includes a second air pressure flow regulating component and a third connecting pipe connected in sequence; The first air pressure flow regulating component and the second air pressure flow component each include a first valve, a detection component and a second valve sequentially connected along the flow diversion direction, and the detection component includes a pressure gauge and a flow meter; Step 2: heating and cleaning; Put the first pair of pipes, the sample dummy and the second pair of pipes into an oven for heating; The temperature of the oven is 110°C, and the hot baking time of the oven is 60 minutes; Step 3, heating the sample branch and the blank branch; Wrap a heating tape around the outside of the sample branch and the blank branch for heating. The heating temperature of the heating tape is 70±2℃. The first air pressure flow regulating component and the second air pressure flow regulating component control the flow rate to 0.9L / min-1.1L / min; Step 4, connecting the ends of the second and third connecting pipes to the organic matter adsorption tube for sampling; The nitrogen supply pipeline ventilates the sample branch and the blank branch for 1 hour, and the adsorption tubes connected to the second and third connecting pipelines collect gas for 1 hour; Test the organic adsorption tube to ensure that there is no total hydrocarbon in the sample branch and the blank branch; Step 5, remove the sample simulation part, install the test sample, and connect the two ends of the test sample to the first butt joint pipe and the second butt joint pipe respectively; Keep the heating temperature of the heating belt at 70±2℃; The first air pressure flow regulating component and the second air pressure flow regulating component control the flow rate to 0.9L / min-1.1L / min; Connect the ends of the second and third pair of pipes to the organic matter adsorption tubes for sampling; The nitrogen supply pipeline ventilates the sample branch and the blank branch for 1 hour, and the adsorption tubes connected to the second and third connecting pipelines collect gas for 1 hour; Step six, place the organic adsorption tube on the sample plate of TD-GCMS for testing.

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